CN103642581A - Sea-buckthorn leaf oil and preparation method thereof - Google Patents

Sea-buckthorn leaf oil and preparation method thereof Download PDF

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CN103642581A
CN103642581A CN201310583190.XA CN201310583190A CN103642581A CN 103642581 A CN103642581 A CN 103642581A CN 201310583190 A CN201310583190 A CN 201310583190A CN 103642581 A CN103642581 A CN 103642581A
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sea
solvent
buckthorn
oil
leaf oil
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CN103642581B (en
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李云飞
王秀梅
乔进才
郝桂莲
孙官印
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Inner Mongolia Seabuckthorn Innovative Application Technology Research Co ltd
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Ordos Tianjiao Resource Development Co ltd
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Abstract

The invention discloses sea-buckthorn leaf oil and a preparation method thereof, wherein the sea-buckthorn leaf oil is rich in trans-palmitoleic acid and has the content of 8-10% by mass percent, and the preparation method of the sea-buckthorn leaf oil is mature in process and suitable for industrial mass production.

Description

A kind of sea-buckthorn leaf oil and preparation method thereof
Technical field
The invention belongs to medical technical field, relate to a kind of sea-buckthorn leaf oil and preparation method thereof, be particularly rich in sea-buckthorn leaf oil of trans Zoomeric acid and preparation method thereof.
Background technology
The sea buckthorn resources of China accounts for 90% left and right of global sea-buckthorn total amount, wherein major part is wild scrub growth, since nearly two more than ten years, for checking winds and fixing drifting sand, conserve water and soil, again expanding species many Seabuckthorn Forests, great majority are also the wild kinds of < < Chinese sea buckthorn > >.Sea-buckthorn is dioecian plant, and in wild sea-buckthorn population, the quantity of male plant is much larger than female, and its ratio usually reaches tens to one degree, and the male sea-buckthorn branches and leaves of looking luxuriant.Not only high but also large, except its ecological benefits, seldom there is utility value, utilize in recent years Folium Hippophae sea-buckthorn tea processed, be only a kind of simple processing, and quantity is very little.
On December 23rd, 2011, message-forward position biomedical information net it is reported, the scientist of HSPH of Harvard University (HSPH) and study from the co-worker of other mechanisms a kind of crude substance of finding in milk fat and may greatly reduce the risk of suffering from diabetes B.This compound, trans Zoomeric acid, is a kind of lipid acid all containing in milk, cheese, Yoghourt and butter.Because human body can not oneself produce, so can only absorb from diet.By the attached Vasculocardiology Deparment associate professor Dariush Mozaffarian of Brigham Women's Hospital of medical college of HSPH epidemiology Xi He Harvard University and HSPH genetics system and complex disease section directors
Figure BDA0000417814220000011
professor J.S.Simmons leader's researchist reports title in < < Annals of Internal Medicine > >, foundation Epidemiological Evidence in recent years shows, is rich in the risk that trans Zoomeric acid may reduce diabetes B and metabolic disturbance diseases in diet.Fitness guru advises reducing whole-milk goods conventionally, but finds that milk fat contains trans Zoomeric acid.3,736 experimenters have been included in this research in, the Hazard Factor of following up a case by regular visits to assess the elderly's cardiovascular disorder of the 20 years behavior phases of going forward side by side.With 1992, store blood sample test as the metabolism risk factors such as blood sugar and Regular Insulin, blood circulation lipid acid (comprising trans Zoomeric acid) level, the progress of follow-up investigation experimenter diabetes B.At baseline, adjust after other Hazard Factor, the high-caliber trans Zoomeric acid of blood circulation to blood cholesterol, marker of inflammation, insulin level, insulin sensitivity etc. in more health level is relevant.Between follow-up period, in blood the higher experimenter of trans Zoomeric acid level to suffer from the risk of diabetes lower, compare the trans Zoomeric acid experimenter's of highest level Risk Reduction 60% with the trans Zoomeric acid experimenter (1/5) of minimum level.The main author Mozaffarian of research says, still need other observational study and controlled trial of the conclusion of this observational study confirms, but this correlation degree is startling.This is the research of assessing first relation between trans Zoomeric acid and diabetes risk.Still do not know at present that this natural trans fatty acid possibility that is present in dairy fat imitates the part biological effect of cis Zoomeric acid (a kind of lipid acid that human body self produces).Experimentation on animals shows that cis Zoomeric acid can prevent diabetes.
According to existing domestic and international scientific and technical literature, record, natural trans fatty acid exists only in the fatty tissue and milk-product of ruminating animal (ox, sheep).In addition, the trans Zoomeric acid in milk-product is limited, and multiple because natural trans fatty acid wherein has, in the majority is antiform oleic acid, is secondly trans-linoleic acid, linolenic acid.
Summary of the invention
The object of this invention is to provide a kind of sea-buckthorn leaf oil and preparation method thereof.Be particularly related to sea-buckthorn leaf oil being rich in trans Zoomeric acid and preparation method thereof.
Key problem in technology of the present invention is: utilize the blade of a large amount of male sea-buckthorns to do deep processing, first extract the leaf oil in blade, now also just completed the thorough degreasing process of blade, make sea-buckthorn leaf oil.The natural trans Zoomeric acid that contains by mass percentage 8-10% in sea-buckthorn leaf oil.
For achieving the above object, the preparation method's that adopts technical process is as follows in the present invention:
(1) receiving leaf is dried
(2) cured leaf leaches;
(3) solvent is reclaimed in evaporation;
(4) desolvation;
(5) supercritical CO 2extraction, again purifying.
Preferably, the preparation method of sea-buckthorn leaf oil of the present invention comprises following concrete technological process:
(1) receiving leaf is dried;
By the male strain fresh leaves of sea-buckthorn collecting in annual 7,8, September through drum-type hot blast wink-dry (blade is heated to 80-90 ℃, 8-10 second); The warehousing of cured leaf dress gunnysack.
(2) cured leaf leaches;
Cured leaf transports input batch extractor, 5m by spiral conveyor 3extractor adds cured leaf 400-500kg.Close batch extractor, start vacuum pump, extract air in tank out, during reach-0.08Mpa of vacuum, close all valves in respective line, start hydrocarbon pump, solvent is injected to batch extractor.Equipment chuck leads to steam, is warming up to 45-50 ℃, at interval of 15 minutes, stirs 10 minutes; Suction filtration after 40-60 minute, the high density mixing oil suction evaporating pot that suction filtration is obtained, every batch materials repeats to leach 3 times.
(3) solvent is reclaimed in evaporation;
In evaporating pot, be high density mixing oil, with air compressor machine, vacuumize decompression, in chuck, logical 90 ℃ of hot water heat up material, impel solvent evaporation, the solvent gas of discharging compresses and liquefies through compressor again, and the solvent after liquefaction reclaims through condenser, flows into solvent tank and recycles.In vapor can, pressure drops to after normal pressure, by the crude oil input crude oil tank reclaiming in evaporating pot after solvent.(its amount of residual solvent of crude oil is now higher, about 50-200mg/kg scope)
(4) desolvation;
Crude oil is processed through scraper-type traditional vacuum thin-film evaporator, spread to liquid film as thin as a wafer, in vacuum environment and be warming up to 60-70 ℃, obtain purifying sea-buckthorn leaf oil.(now in crude oil, the remaining solvent overwhelming majority is removed, its amount of residual solvent can≤1.0ppm)
(5) purifying again;
Step (4) gained purifying sea-buckthorn leaf oil, because including chlorophyll, unsatisfactory on its color and luster, through supercritical CO 2the purification by liquid extraction again of unit, removes chlorophyll, obtains end product sea-buckthorn leaf oil, its golden appearance.(sea-buckthorn leaf oil is containing the natural trans Zoomeric acid of mass percent 8-10%).
In described technical process, solvent is liquid, is apolar substance, approaches with oily specific inductivity, is convenient to oil extraction.Described solvent is selected from the organic solvents such as butane, propane, and preferred described solvent is butane.
Embodiment
Embodiment mono-:
(1) receiving leaf is dried;
By the male strain fresh leaves of sea-buckthorn (4T/h) collecting in annual 7,8, September through drum-type hot blast wink-dry (blade is heated to 80 ℃, 8-10 second); The warehousing of cured leaf (25kg) dress gunnysack.
(2) cured leaf leaches;
Cured leaf (450kg) is transported and is dropped into 5m by spiral conveyor 3batch extractor, (450kg/ time).Close batch extractor, start vacuum pump, extract air in tank out, during reach-0.08Mpa of vacuum, close all valves in respective line, start hydrocarbon pump, solvent is injected to batch extractor.Equipment chuck leads to steam, is warming up to 45 ℃, at interval of 15 minutes, stirs 10 minutes; Suction filtration after 60 minutes, the high density mixing oil 2000L that suction filtration is obtained, every batch materials repeats to leach 3 times, and the high density mixing oil 4500L obtaining for three times is merged to suction evaporating pot.
(3) solvent is reclaimed in evaporation;
In evaporating pot, be high density mixing oil, with air compressor machine, vacuumize decompression, in chuck, logical 90 ℃ of hot water heat up material, impel solvent evaporation, the solvent gas of discharging compresses and liquefies through compressor again, and the solvent after liquefaction reclaims through condenser, flows into solvent tank and recycles.In vapor can, pressure drops to after normal pressure, by the crude oil 80L input crude oil tank reclaiming in evaporating pot after solvent.
(4) desolvation;
Crude oil is processed through scraper-type traditional vacuum thin-film evaporator, spread to liquid film as thin as a wafer, in vacuum environment and be warming up to 60 ℃, obtain purifying sea-buckthorn leaf oil 65L.
(5) purifying again;
Step (4) gained purifying sea-buckthorn leaf oil, because including chlorophyll, unsatisfactory on its color and luster, through supercritical CO 2the purification by liquid extraction again of unit, removes chlorophyll, obtains end product Folium Hippophae (50L), its golden appearance.
Through liquid chromatograph-area normalization method, measuring the natural trans Zoomeric acid content of end product sea-buckthorn leaf oil is 8.1g/100g, and to account for the per-cent of sea-buckthorn leaf oil be 8.1% to natural trans Zoomeric acid as calculated.
Embodiment bis-
(1) receiving leaf is dried;
By the male strain fresh leaves of sea-buckthorn (4T/h) collecting in annual 7,8, September through drum-type hot blast wink-dry (blade is heated to 90 ℃, 8-10 second); The warehousing of cured leaf 25kg dress gunnysack.
(2) cured leaf leaches;
Cured leaf 450kg transports input batch extractor, (450kg/ time) by spiral conveyor.Close batch extractor, start vacuum pump, extract air in tank out, during reach-0.08Mpa of vacuum, close all valves in respective line, start hydrocarbon pump, solvent is injected to batch extractor.Equipment chuck leads to steam, is warming up to 50 ℃, at interval of 15 minutes, stirs 10 minutes; Suction filtration after 40 minutes, the high density mixing oil 2000L that suction filtration is obtained, every batch materials repeats to leach 3 times, and the high density mixing oil 4500L obtaining for three times is merged to suction evaporating pot.
(3) solvent is reclaimed in evaporation;
In evaporating pot, be high density mixing oil, with air compressor machine, vacuumize decompression, in chuck, logical 90 ℃ of hot water heat up material, impel solvent evaporation, the solvent gas of discharging compresses and liquefies through compressor again, and the solvent after liquefaction reclaims through condenser, flows into solvent tank and recycles.In vapor can, pressure drops to after normal pressure, by the crude oil 70L input crude oil tank reclaiming in evaporating pot after solvent.
(4) desolvation;
Crude oil is processed through scraper-type traditional vacuum thin-film evaporator, spread to liquid film as thin as a wafer, in vacuum environment and be warming up to 60 ℃, obtain purifying sea-buckthorn leaf oil 55L.
(5) purifying again;
Step (4) gained purifying sea-buckthorn leaf oil, because including chlorophyll, unsatisfactory on its color and luster, through supercritical CO 2the purification by liquid extraction again of unit, removes chlorophyll, obtains end product sea-buckthorn leaf oil 45L, its golden appearance.
Through (liquid chromatograph-area normalization method), measuring the natural trans Zoomeric acid content of end product sea-buckthorn leaf oil is 7g/100g, and to account for the per-cent of sea-buckthorn leaf oil be 7% to natural trans Zoomeric acid as calculated.
The part that the present invention does not relate to all prior art that maybe can adopt same as the prior art is realized.

Claims (5)

1. a sea-buckthorn leaf oil, is characterized in that containing by mass percentage in sea-buckthorn leaf oil the natural trans Zoomeric acid of 8-10%.
2. sea-buckthorn leaf oil claimed in claim 1, is characterized in that the preparation method of described sea-buckthorn leaf oil comprises the following steps:
(1) receiving leaf is dried;
(2) cured leaf leaches;
(3) solvent is reclaimed in evaporation;
(4) desolvation;
(5) supercritical CO 2extraction, again purifying.
3. sea-buckthorn leaf oil claimed in claim 2, is characterized in that the preparation method of described sea-buckthorn leaf oil comprises the following steps:
(1) receiving leaf is dried;
By the male strain fresh leaves of sea-buckthorn collecting in annual 7,8, September, through drum-type hot blast wink-dry, blade is heated to 80-90 ℃, 8-10 second; The warehousing of cured leaf dress gunnysack;
(2) cured leaf leaches;
Cured leaf transports input batch extractor, 5m by spiral conveyor 3extractor adds cured leaf 400-500kg; Close batch extractor, start vacuum pump, extract air in tank out, during reach-0.08Mpa of vacuum, close all valves in respective line, start hydrocarbon pump, solvent is injected to batch extractor; Equipment chuck leads to steam, is warming up to 45-50 ℃, at interval of 15 minutes, stirs 10 minutes; Suction filtration after 40-60 minute, the high density mixing oil suction evaporating pot that suction filtration is obtained, every batch materials repeats to leach 3 times;
(3) solvent is reclaimed in evaporation;
In evaporating pot, be high density mixing oil, with air compressor machine, vacuumize decompression, in chuck, logical 90 ℃ of hot water heat up material, impel solvent evaporation, the solvent gas of discharging compresses and liquefies through compressor again, and the solvent after liquefaction reclaims through condenser, flows into solvent tank and recycles; In vapor can, pressure drops to after normal pressure, by the crude oil input crude oil tank reclaiming in evaporating pot after solvent;
(4) desolvation;
Crude oil is processed through scraper-type traditional vacuum thin-film evaporator, spread to liquid film as thin as a wafer, in vacuum environment and be warming up to 60-70 ℃, obtain purifying sea-buckthorn leaf oil;
(5) purifying again;
Step (4) gained purifying sea-buckthorn leaf oil, because including chlorophyll, unsatisfactory on its color and luster, through supercritical CO 2the purification by liquid extraction again of unit, removes chlorophyll, obtains end product sea-buckthorn leaf oil.
4. sea-buckthorn leaf oil claimed in claim 3, is characterized in that the solvent in the preparation method of described sea-buckthorn leaf oil is organic solvent.
5. sea-buckthorn leaf oil claimed in claim 4, is characterized in that the solvent in the preparation method of described sea-buckthorn leaf oil is butane.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109576064A (en) * 2018-12-27 2019-04-05 国家海洋局第三海洋研究所 The method for preparing trans- palmitoleic acid is separated from fish oil
CN110295086A (en) * 2019-07-03 2019-10-01 青海伊纳维康生物科技有限公司 A method of purifying palmitoleic acid from hippophae rhamnoides fruit oil

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109576064A (en) * 2018-12-27 2019-04-05 国家海洋局第三海洋研究所 The method for preparing trans- palmitoleic acid is separated from fish oil
CN110295086A (en) * 2019-07-03 2019-10-01 青海伊纳维康生物科技有限公司 A method of purifying palmitoleic acid from hippophae rhamnoides fruit oil
CN110295086B (en) * 2019-07-03 2020-11-13 青海伊纳维康生物科技有限公司 Method for purifying palmitoleic acid from sea buckthorn fruit oil

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